Method of producing hydrated calcium silicate minerals and products thereof



p -24,1940. G. M. THOMSON ET AL 2 215,891

METHOD OF PRODUCING HYDRATED CALCIUM SILICATE MINERALS AND PRGDUCTS THEREOF Filed NOV. 12, 193B |Ill D lA/VE/VTO/FJ:

GEORGE M. THOMSON 'm/ 20L TA/v 59051.5)

Patented Sept. 24, 1940 2,215,891

METHOD OF PRODUCING HYDRATED CAL- CIUM SILICATE MINERALS AND Paon- UCTS THEREOF George Miller Thomson, Caledonia, .Ontario. and Zoltan Erdeley, Brantford, Ontario, Canada, assignors to Gypsum, Lime and Alabastine, Canada, Limited, Paris, Ontario, Canada Application November 12, 1938, Serial No. 240,000 r 1 9 Claims. (Cl. 106'-24) 6 tent can be bonded into hard masses by mixing necessary for quick dissolving to replace that exwith it small amounts of hydrated lime and tracted by the silica, so that any degree of'conenough water to provide a damp mixture which is centration may be maintained. The lime should subjected to a pressure of about 2000 lbs. per be hydrated in large quantities and thoroughly 7 square inch and then indurated under a steam mixed beforehand. If uniformity is maintained 10 pressure of 120 lbs. per square inch for a period for both silica and hydrated lime, identical re- 10 of eighthours. In the Komnick process, which sults are obtained under uniform operating conas been used for many years, the damp mixture ditions of temperature, pressure, and the like. is heated for about 20 minutes at about 50 lbs. The method for producing structural materials steam pressure, in a mixing drum. revolving on includes three stages in each of which the con-' a horizontal axis, prior to compression and subsecentration of lime in the solution surrounding 15 quent induration. The product of such a process the reacting silica particles is closely controlled. has a density of about 129 lbs. per cubic foot and In the first sta e a s f l yp hydrated a compressive strength of about 6000 lbs. per cium silicate is formed. In the second stage a square inch. crystalline hydrated calcium silicate is formed Many attempts have been made to produce durand in the third stage the material is changed 20 able light weight materials, utilizing this limeto a hard gel type or amorphous hydrated calsilica reaction, but insofar as applicants are cium silicate, which is believed to be gyrolite, aware no commercial method has heretofore been 2CaO.3SiO2.2I-I2O, in structural form. available or known for producing such products A form of apparatus for carrying out the methof uniform densityor compressive strength. 0d is more or less diagrammatically illustrated 25 The object of the present invention is to proin the accompanying drawing in which vide light weight durable materials of desired Figure llis the crystal generator with the lime density and compressive strength and a method concentration measuring device,

whereby such products may be synthetically pro- Figure 2 is the induralting autoclave and duced in line production and in any desired Figure 3 is a mold with drainage facilities. 30 structural form. The invention also contem- A generator tank I is provided with a central plates the production of synthetic hydrated calshaft 2 driven from a pulley 3 and carrying agi cium silicate in other than structural forms. tating or stirring means, represented by a metal It is well known that there is a substantial ribbo 4 arranged to direct material to a bottom number of hydrated calcium silicates containing disch rge 5. 6 represents a main charging port varying proportions of lime, silica and water. and 6' an inlet foblime. I is a steam inlet, 8 After prolonged and intensive research, applia steam exhaust outlet and 9 a steam pressure cants have developed a method whereby some of guage. The device 'for measuring lime concensuch minerals can be produced synthetically and tration of the solution consists of an electrode I0 commercially in structural and other forms of a having two polesJ/ referably of platinum, im- 40 ,f porous character, containing innumerable submersed in the. soluti n in the generator and conmicroscopic pores throughout the mass. The nected to a constant source II of alternatingelecpores orvoid spaces may, represent as much as tric current witha meter i2 in the circuit. The 90% of the total volume ofthe'mass in the lightest meter may indicate the current flow in milliweight products, and the pore sizes afford very amperes or'theresistance to currentflow in ohms. 45 low heat conductivity. Such instruments are commercially available. The silica employed is uniformly ground and Alternating current jiS used to prevent coating of at least 90% should pass through 200 mesh the electrodes. g screen. The finer' the particles ofsilica the faster The ind rating dlevice consists of the autoclave 3 the reaction. High calcium type lime with a low l3 of the ype' lcommonly used formaking sand percentage of impurities is used. It should be lime brk an has a track for receiving cars crushed to pass a 1 /2" screenropening. It is hycarryin the molds, a removable pressure tight drated in an excess of water/preferably 5 to 6 door, a steam supply pipe and a trap for condenparts of water to l of lime, and at a temperature, sation. It may be provided with a bleeding line I4 adapted to permit inflow of air to prevent This invention relates to the production of hydrated calcium silicates and light weight and other products thereof.

It is well known that sand of high silicate c0n-' preferably not less than 200 F. to insure very fine particles of hydrated lime. As hot water has a very low capacity for dissolved lime, and as silica combines rapidly with dissolvedlime at high temperatures, very fine lime particles are formation of vacuum during the pressure reduction period.

The mold i5 is provided with a perforated bottom 16 for drainage purposes and a detachable liner i! capable of acting as a filter to release the solution.

In operation the generator is preferably first heated to about the boiling point of water. The concentration measurement device is adjusted to place. The: generator is charged with the finely divided silica and a hot aqueous lime solution having a concentration of not more than 99% nor lessthan 81% of saturation. It isessential to maintain the lime concentration withinthe limits stated during this stage of the operation.

-Th'epreferred operating range is 90 to. 95% of saturation. In order that'the silica may remain freely suspended under the influence of the agitator, sufiicient water should be present, in the proportion of, say three pounds of water per pound of silica. The temperature within the generator is raised to the desired point, say 338 F., .the equivalent of 100 lb. steam pressure, bythe admission of steam or by other heating means. The lime combines with silica and to maintain the required concentration lime is fed into the solution in the generator Eat a slowly accelerating rate as the temperature rises. A soft gel type hydrated silicate is formed during this stage. It is important to avoid the presence of excessive amounts of undissolved lime as it causes flocculation with silica particles, which removes appre ciable portions ,of the lime and silica from the action of the surrounding lime solution. By reading the. measuring instrument the rate of feeding lime is readily controlled to maintain the required concentration of lime. Not more than two-thirds of the silica is causedto combine with lime in this soft gel forming period. The

50. and grow. "Some of the end mineral after induration, to be later described, being gyrolite (2CaO.3SiO2.2HzO) the theoretical proportion of lime and silica is .622 lime to 1 of silica by weight. Slightly more than half of the calculated amount of lime is added during this stage.

The lime concentration of the solution is now r d t an main ains some attached and emanating from minute silica remnants and appearing under the' microscope as burr-like clusters, andcthers emanating. as spikes from certain faces of silica particles. It may be observed that the's'eburr-like clusters act as fenders to prevent close'packing of the crystals in their disordered relationship in the mass. The temperature is maintained until there is a pronounced drop in the concentration as indicated by the instrument. The crystal growing period is then complete and the heating is discontinued before the concentration is allowed to drop below of saturation and preferably earlier.

The material is then drained to remove the lime water. This may be accomplished in a drainage or settling tank or by discharging the mass directly into molds provided with drainage facilities as described. The charged molds are run into the indurating autoclave and thematerial is consolidated into structural form by main- .tenance of a live steam pressure of say, pounds for a period of, for example, 5 to 8 hours or longer.

The indurated product thus formed has high and uniform compressive-m. the lightest weight materiaL. about l2'lbs. per cubic foot, consists practically entirely 'af-igmiite interspersed with minute pores,

While as the weight per cuhicaliltzlhcreues the proportion of unccmbined silica increases 'and the gyrolite decreases. I'n the heavy material, say 55 1bs.'per cubic foot, while-theproportion of gyrolite is much lessyit is still sufflcient to providenot exceed that which can combine with silica to form gyrolite. I

When unconsolidated small particles of gyrolite' are required rather than theshaped-structural products, the formation of the soft gel type silicate is continued as previously described until all of the lime has been fed to thegenerator. As the heating is continuedtheiime concentration drops below 81% of saturation, and fine unconsolidated particles of. gyrolite .IXG formed.

i This application is a continuation in part of application Serial Number 97,410'iiled August 22,

We claim: i I

1. In the production of hydrated calcium silicates, the method which comprises suspending finely divided silica-in a lime solution, which is about 90% saturated, under steam pressure and while maintaining said pressure adding lime to maintain substantially that degree of lime concentrationin said solution. 7

2. In the production of hydrated calcium silicate' products, the method which comprises'suspending finely divided silica in a solution of lime under steam pressure,- adding lime to maintain a predetermined lime concentration in said solution while forming one type-of said silicate, thereafter adding lime .to maintain a" different predetermined lime concentration in said solution to form another type of said silicate'and maintainthroughout the. reaction period,- .*3;.-A 'niet'hodas setforth in" silicate. onnes *isldrained em'old'ed and the molded product is-haLrdene under steam presinduratin'g the same under steam pressure to harden the material.

5. A method of makinglight weight insulating blocks, comprising the steps of finely pulverizing silica material. hydrating high calcium lime in an excess of water,suspending silica particles in -lime solution in a -he'ated-..zone, adding thereto lime to produce and maintain a. lime concentration not less than 81 nor; more than 90% saturation while forming a soft-gel type of silicate, raising the lime concentration to saturation to grow silicate crystals,'draining and shaping the mass ,and hardening the shapes under steam pressure.

he reactingv mass under; steam pressure.

'total lime contentof the finis'hediprodiict does 6. A method of making light weight structural materials consisting essentially of hydrated calcium silicate, including the steps of finely pulverizing silica material, hydrating lime in an excess of water, measuring the lime and the silicate be combined, the proportion of lime being not more than .622 lb. per pound of silica, suspending the silica. in lime solution, heating the mass, adding thereto more than 50% of the lime .while maintaining the lime concentration of the solution at about 90% of saturation to form a soft gel type silicate, adding the balance of the lime whilemaintaining thesolution saturated to form crys- 8. A method as set forth in claim 4 wherein the lime does not exceed .622 pound'per pound of silica-and in excess of 50% of the lime is added prior to the crystal growing period.

9. A three stage method for making hydrated 'siiicate products from finely divided silica suspended'in a solution of lime under steam pressure,

- comprising a soft gel forming stage in which the stage in which the lime concentration of the solution is maintained at saturation and an indurating stage in which the crystalcontaining molded mass from which the lime solution has been drained is heated under steam pressure.

GEORGE MILLER THOMSON. ZOLTAN ERDELEY.

CERTIFICATE OF CORRECTION.

Patent no. 2,21 ,891. September 21;, 191p.

GEORGE MILLER THOMSON, ET AL.

It is hereby certified that error appears in the printed specification of the above numbered patent requiring v correction as follows: Page 2, second column, line 70, claim 5, for" 90% read -99% and that the said Letters Patent should be read with this correction therein that the same may conform to the record of the case in the fatent Office.

Signed and sealed this 12th day of No ember, A. D. 1914.0.

v Henry Van Arsdale,

(Seal) Acting Commissioner of Patents. 

